تفاعل #816425

ord-c567e8fa42ad4663ad7a0baaf04387ee

المذيبات

ظروف التفاعل

درجة الحرارة
150°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe THF was evaporated
  2. 2
    استخلاصthe residue was extracted with DCM
  3. 3
    أخرىThe mixture was evaporated
  4. 4
    أخرىthe residue was triturated in petroleum ether
  5. 5
    أخرىthe solvent was decanted

الإجراء التجريبي

Potassium tert-butoxide (0.845 g, 10.56 mmol) was added to a solution of N-(tert-butyl)-1-phenylmethanesulfonamide (1.2 g, 5.28 mmol) and diethyl oxalate (0.85 mL, 6.33 mmol) in THF (8 mL) and the mixture was heated at 150° C. for 15 mins in a microwave reactor. The reaction mixture was acidified with 1M HCl, the THF was evaporated and the residue was extracted with DCM. The mixture was evaporated, the residue was triturated in petroleum ether and the solvent was decanted to give the title compound (7 g, 63%) as a solid; 1H NMR (500 MHz, CDCl3): δ 7.44-7.32 (m, 5H), 3.90 (br s, 1H), 1.36 (s, 9H); Mass Spectrum: M−H+280

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07582629B2uspto-grants-2009_09